Hydrochloric Acid → HCID 66917896, compound

HRID 1593371Notes

Reaction equation

HRID 1593371 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[N:9]2[CH2:14][CH2:13][N:12]([CH2:15]/[CH:16]=[CH:17]\[CH2:18][O:19][CH2:20][C:21]([OH:23])=[O:22])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[ClH:31].[CH:32](O)([CH3:34])[CH3:33]>>[ClH:31].[ClH:31].[CH:32]([O:22][C:21](=[O:23])[CH2:20][O:19][CH2:18]/[CH:17]=[CH:16]\[CH2:15][N:12]1[CH2:13][CH2:14][N:9]([CH:8]([C:24]2[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=2)[C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[CH2:10][CH2:11]1)([CH3:34])[CH3:33]

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 3776Isopropanol2×HCID 10150997HCID 10150997, compound

Product 1

HCID 66917896HCID 66917896, compoundYield 75.85%

Conditions

Temperature
27.5 °C

Procedure

To a stirred solution of {4-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-yl}-(Z)-but-2-enyloxy}acetic acid (1.0 g, 0.0024 mol) in isopropyl alcohol (20 ml), is added a solution of anhydrous HCl in isopropyl alcohol till pH of solution is 1-2. The solution is refluxed for around 2 hrs, cooled to 25-30° C. and stirred for 4 hrs. The crystallized solid is filtered, washed with isopropyl alcohol (2×5 ml), and dried in oven at 60-65° C. to get product 0.968 g (75.85% yield).

Workup

  1. temperatureThe solution is refluxed for around 2 hrs
  2. filtrationThe crystallized solid is filtered
  3. washwashed with isopropyl alcohol (2×5 ml)
  4. customdried in oven at 60-65° C.

Sources & evidence

ORD record
ord-4e69c62620744789897514737cc43f8b
Source dataset
uspto-grants-2007_11
Patent number
US07297697B2

Reaction notes

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